自制花椒调味油中11种真菌毒素的研究分析

Analysis of 11 Kinds of Mycotoxins in Homemade Zanthoxylum bungeanum Seasoning Oil

目的:确认自制花椒调味油在食用及储存过程中是否产生11种常见的真菌毒素,采用超高效液相色谱-串联质谱法分析检测花椒油中的真菌毒素。方法:花椒油样品采用70%的甲醇水超声提取,经多功能净化柱净化,Waters ACQUITY UPLC HSS T3C18色谱柱分离,以0.2%氨水溶液和乙腈梯度洗脱,利用串联三重四极杆质谱多反应模式、负离子监测方式检测,并采用内标法及外标法综合定量。结果:11种真菌毒素有较好的线性范围,进行3种不同浓度水平的加标回收实验,其回收率为68.5%~102.5%,相对标准偏差(RSD)为0.81%~6.87%,检出限为0.02~0.10μg/kg,定量限为0.15~2.00μg/kg,并进行了真菌毒素质控样的测定,测定值在参考值允许范围内。结论:花椒油样品中均未检出11种真菌毒素,在食用过程中是安全的,该方法具有灵敏度高、重复性好、准确度高、检测速度快的优点且样品前处理操作便捷,适用于花椒油中11种真菌毒素的检测。

Objective：To confirm whether Zanthoxylum bungeanumseasoning oil produces 11 kinds of common mycotoxins in the process of eating and establish a simultaneous detection method for the determination of 11 kinds of mycotoxins in Zanthoxylum bungeanum seasoning oil by ultra performance lliquid chromatography-tendem mass spectrometry（UPLC-MS/MS）.Methods：After extraction by70% methanol and purification by multifunction cleaning column,the mycotoxins of Zanthoxylumoil are separated by a chromatographic column of Waters ACQUITY UPLC HSS T3 C18 by the gradient elution of mobile phase with 0.2%ammonia solution and acetonitrile.The mass spectrometry is conducted by using negative（ESI-）electrospray ionization and multi-reactions monitoring（MRM）models,internal and external standard method are used to quantify.Results：The 11 mycotoxins have good linear relationship with peak areas.The recovery experiments are carried out through three concentration levels of low,medium and high concentration,the recovery rates are in the range of 68.5%~102.5%,the relative standard deviation（RSD）is in the range of 0.81%~6.87%,the limit of detection is in the range of 0.02~0.10μg/kg,the limit of quantification is in the range of 0.15~2.00μg/kg.Through the determination of the quality control of mycotoxin,the detection value is within the reference value.Conclusion：11 kinds of mycotoxins are not detected in Zanthoxylum bungeanum seasoning oil samples.The method has the advantages of high sensitivity,good repeatability,high accuracy,convenient operation and quick detection speed,is applicable for the detection of 11 kinds of mycotoxins in Zanthoxylum bungeanumseasoning oil.